EP2183193B1 - Einphasiges hydraulisches bindemittel, herstellungsverfahren und damit hergestellter baustoff - Google Patents

Einphasiges hydraulisches bindemittel, herstellungsverfahren und damit hergestellter baustoff Download PDF

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EP2183193B1
EP2183193B1 EP08784792.7A EP08784792A EP2183193B1 EP 2183193 B1 EP2183193 B1 EP 2183193B1 EP 08784792 A EP08784792 A EP 08784792A EP 2183193 B1 EP2183193 B1 EP 2183193B1
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silicate
hydraulic binder
calcium
connectedness
binder
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German (de)
English (en)
French (fr)
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EP2183193A1 (de
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Günter BEUCHLE
Peter Stemmermann
Uwe Schweike
Krassimir Garbev
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Karlsruher Institut fuer Technologie KIT
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Karlsruher Institut fuer Technologie KIT
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Classifications

    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B7/00—Hydraulic cements
    • C04B7/345—Hydraulic cements not provided for in one of the groups C04B7/02 - C04B7/34
    • C04B7/3453—Belite cements, e.g. self-disintegrating cements based on dicalciumsilicate
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
    • C04B28/18—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing mixtures of the silica-lime type
    • C04B28/186—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing mixtures of the silica-lime type containing formed Ca-silicates before the final hardening step
    • C04B28/188—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing mixtures of the silica-lime type containing formed Ca-silicates before the final hardening step the Ca-silicates being present in the starting mixture
    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/00034—Physico-chemical characteristics of the mixtures
    • C04B2111/00215—Mortar or concrete mixtures defined by their oxide composition
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P40/00—Technologies relating to the processing of minerals
    • Y02P40/10—Production of cement, e.g. improving or optimising the production methods; Cement grinding

Definitions

  • the invention relates to a single-phase hydraulic binder, a mixture containing such a binder, processes for the preparation of the binder and the mixture and a building material, which was prepared with the binder or the mixture.
  • the hydraulic reactivity describes the reaction of a binder with water to form a solid material.
  • the definition of this process is based on the previously known hydraulic binders such as Portland cement. After Härig, Günther, in Klausen, Technologie der Bauscher, CF Müller Verlag, Heidelberg, 1996, p. 53 , hydraulic binders harden after addition of water both in air and under water.
  • Cement is a hydraulic binder which, when mixed with water to a paste (Ze mentleim ), stiffen automatically due to chemical reactions between the water and the compounds present in the cement and hardens to cement stone . Stiffening and hardening depend neither on drying nor on reactions with the CO 2 from the air. The reaction therefore takes place both in air and under water.
  • latent hydraulic (so-called pozzolanic) binders are known. According to Härig (see above) these harden after addition of water only in the presence of an activator. To start the setting reaction then, for example, lime hydrate or Portland cement is added; however, there is no independent reaction.
  • a typical example of such latent hydraulic binders are blast furnace slags with a mass ratio (CaO + MgO): SiO 2 of> 1 (EN 197-1: 2000, Section 5.2.2).
  • silicate-based hydraulic binders do not contain any molecular water, their hydraulic components contain no hydrogen and the hydraulic components in their empirical formula consist predominantly of crystalline (earth) alkali silicates.
  • the silicate anions of the hydraulically active phases decrease HFW Taylor, The chemistry of cement, Academic Press, London 1964, p. 2f , in the form of individual isolated or monomeric silicate tetreaser before (Q 0 ).
  • the exception is the rare phase belinite, which is a ring silicate containing chlorine.
  • Belinit each silica tetrahedron is linked to two other silicate tetrahedra via common oxygen (Q 2 ).
  • All previously known silicate-based hydraulic binders have a molar ratio CaO: SiO 2 of at least two.
  • Types 2 and 3 water glasses and geopolymers, are only conditionally to be seen as hydraulic binders in the sense of the definition given at the outset, since they are either already present as a solution, ie not solid, or do not harden under water because of their high water solubility (alkali metal silicates). or are non-reactive as solids and require additives such as CEM I or caustic to initiate the hydraulic reaction. They require for their production both special starting materials and each more complex process steps, whereby their production is expensive. At the same time their compatibility with various additives is extremely limited due to the very high pH and the usually very slow reaction rate can not be effectively influenced, in particular not be accelerated. Because of the limited processability (slow hardening, strong alkaline reaction) and the low strength, their range of applications is therefore limited.
  • the best known and most commonly used hydraulic binder is cement, especially Portland cement.
  • the necessary for the production of the precursor cement clinker at temperatures up to about 1450 ° C combustion process is after HFW Taylor, Cement chemistry, Academic Press, London 1990, p. 64f , with a theoretical Reaktiosenthalpie of + 1761 kJ per kg of cement clinker particularly energy-intensive.
  • the lion's share of the energy demand is attributed to the deacidification (or decarbonation) of calcium carbonate derived from limestone, limestone or other calcareous materials.
  • the under Release of CO 2 proceeds with a reaction enthalpy of + 2138 kJ per kg of cement clinker strongly endothermic to the overall reaction.
  • the overall calcium content in Portland cement in general and especially in the precursor clinker can not be significantly reduced, otherwise the hydraulic reactivity decreases greatly.
  • the total calcium content expressed as a molar Ca: Si ratio which is otherwise identical to the molar (CaO) :( SiO 2 ) ratio, is always 3.0 +/- 0.2.
  • the binder matrix of CSH gel present in cement paste made of Portland cement, which originates essentially from the reaction of tricalcium silicate Ca 3 SiO 5 has a molar Ca: Si ratio of 1.7 to 1.8.
  • the excess CaO is present after hydration as Portlandit Ca (OH) 2 .
  • Portlandite contributes only insignificantly to the mechanical stability of the building material. Rather, in the use phase of the cement, portlandite determines the pH value of the building material, which is then at about pH 12.5. Acid attacks are initially buffered by Portlandite; however, if this is used up, for example by CO 2 being converted into CaCO 3 , the pH drops and the CSH gel binder matrix is attacked and decomposed.
  • Portland cement exhibits a high reaction enthalpy during setting, which essentially results from the formation of portlandite, and leads to heat build-up in large, bulky or voluminous components.
  • the evolution of heat per unit time can be reduced by slowing down the reaction conversion by means of grain enlargement, additives or dilution with fly ash. However, this also slows down the development of strength.
  • the strength of cement stone is determined by the main component CSH gel, which accounts for only about 50% by weight. Therefore, the effective energy input to produce the strength constituents of cement from Portland cement is approximately 8600 kJ per kg.
  • the other half of the cement paste essentially calcium aluminate hydrates and portlandite, scarcely contributes to the strength of the material or building material and is an unwanted by-product in terms of strength.
  • the Portlanditmenge can in technical systems subsequently by the admixture of microsilica or latent hydraulic Be reduced substances. Excess portlandite then reacts slowly with the consumption of microsilica to additional calcium silicate hydrates on. This process is however complicated and expensive.
  • C-S-H gels can incorporate calcium in variable amounts. With increasing calcium content, the degree of cross-linking of the associated silicate building units and thus their contribution to the strength of the building material as well as their chemical resistance decreases. In hardened Portland cement stone, the C-S-H gels are present with a molar Ca: Si ratio of 1.7 to 1.8. On the other hand, calcium silicate hydrates exist in a range of the molar Ca: Si ratio of 0.5 to 3.0. This is evidenced by naturally occurring or synthetically produced solids.
  • the mixtures are milled under methanol and then dried at 60 ° C. The dried mass is then pulverized. The resulting mixtures are treated with deionized water and hydration observed at 21 ° C. For this purpose, samples with different degrees of hydration are taken, ground and examined by means of 29 NMR spectroscopy. In particular, the appearance of a species with a degree of crosslinking of Q 3 is observed, which is assigned to a triple chain of silicate units in the resulting calcium silicate hydrate (CSH).
  • CSH calcium silicate hydrate
  • Hasegawa et al. describe in Mechano-radicals produced from ground quartz and quartz glass, Powder Tech. 85 (1995) p. 269 , Changes that occur during the milling of quartz, by detecting defects on the quartz surface by spectroscopic methods. There are no hydraulic binders.
  • the US 3,066,031 A discloses a cementitious binder and a method of making it based on the co-grinding of CaO and oxidic materials such as SiO 2 and / or Al 2 O 3 .
  • the essential ingredient CaO is used in the form of quicklime. By grinding the CaO content is converted to at least 50% in a form that releases less heat when reacted with water as pure CaO.
  • the binder contains in addition to the exciter CaO milled, latent hydraulic aluminosilicates. In the US 4,217,143 A a particular embodiment of this method will be described.
  • the DE 10 2005 018 423 A1 discloses a method for the production of components, wherein the binder used for this purpose are completely hydrated compounds, the solidification of which is not hydraulically but by compression. This silanol units condense with elimination of water.
  • From the DE 22 22 545 B2 is a process for producing a hydrous Calcium silicate of the xonotlite type known, wherein the xonotlite is crystalline.
  • the amorphous precursor described in this patent is due to the hydrothermal production, a non-hydraulically hardening hydrate.
  • the EP 0 500 840 B1 discloses tectoalumosilicate cement and an associated method of manufacture, wherein the tectoaluminosilicate has a degree of crosslinking of Q 4 .
  • the hydraulic hardening of corresponding compounds is not based on the formation of CSH phases.
  • concrete demolition is activated by grinding. However, it is ground so as not to produce a hydraulic product but a product that can be used as a cement raw meal component.
  • the use of concrete demolition also contains in the starting component a sulphate carrier which as a reaction product is likely to prevent the production of a single-phase product.
  • the hydraulic binder according to the invention is a hydraulically active silicate compound containing calcium, silicon and oxygen.
  • Other elements can also be part of the binder and are differentiated according to the nature of their incorporation: alkalis, especially sodium; Alkaline earths, in particular magnesium, or other divalent cations, in particular Fe [+ II] and manganese; Trivalent cations, in particular Al [+ III], are incorporated as M [6] x + sixfold or higher coordinated with oxygen, with the M [6] x + partially replacing the calcium.
  • Tetrahedral oxygen-coordinated elements particularly phosphorus, aluminum or Fe 3+ , form oxygen anions and are incorporated as phosphate, aluminate or ferrate at tetrahedral positions as M [4] y + , replacing silicon at most at 45 atomic%.
  • the amphoteric aluminum is just like magnesium for both variants.
  • the numbers x + and y + indicate the charge of the respective cation.
  • the stoichiometry of the hydraulic binder according to the invention is defined by the range of the molar ratio Ca: Si of 0.2 to 1.5, more preferably of 0.3 and below 1.5.
  • the components oxygen or calcium and other elements provide for the charge balance.
  • M [6] x + O x / 2 or M [4] y + O y / 2 instead of the simple molar Ca: Si ratio, the is identical to the molar (CaO) :( SiO 2 ) ratio, the modified molar ratio [CaO + (x / 2) * (M [6] x + O x / 2 )]: [SiO 2 + M [4] y + O y / 2 ].
  • the content of water is below 3.5 wt.%.
  • the binder proves to be X-ray amorphous by X-ray diffraction (X-ray powder diffractometry), i. it is very much in disorder.
  • Silications consist of oxygen tetrahedra whose center is occupied by a tetrahedrally coordinated silicon.
  • the Silikattetraeder constructed in this way are linked to one another via common oxygen atoms. Silicon atoms can be replaced in higher proportions by aluminum atoms, to a lesser extent by boron, germanium, titanium, iron, beryllium or phosphorus atoms.
  • the structure of the silicates in the hydraulic binder according to the invention is characterized by a variable linking of the tetrahedra.
  • the partial substitution of silicon atoms by atoms of other network formers in particular of aluminum, boron, germanium, phosphorus, iron, beryllium or titanium, is possible. Particularly relevant is the aluminum substitution, the maximum up to a replacement of 45 atom% of the Si can reach through Al.
  • the calcium atoms are in the form of Ca 2+ ions as the binding partner of the negatively charged silicate units. Partial replacement by Na, K, Li, Mg, Sr, Ba, Mn, Fe [+ II], or Al [+ III] atoms is possible.
  • the present invention thus relates to a single-phase hydraulic binder which consists of hydraulically active calcium silicate.
  • this binder contains fewer calcium or less calcium substituting elements, so that the molar ratio [CaO + (x / 2) * (M [6] x + O x / 2 )]: [SiO 2 + M [4 ] y + O y / 2 ] is lower.
  • This hydraulic binder is made by grinding from raw materials that are produced on average at lower temperatures than cement clinker, thus reducing energy and carbon dioxide emissions.
  • the present invention further relates to a mixture which comprises a proportion of the single-phase hydraulic binder according to the invention.
  • the proportion is preferably at least 10% by weight, particularly preferably at least 25% by weight, in particular at least 50% by weight.
  • the setting or curing takes place, as known from Portland cement, by mixing with water and optionally under water.
  • the hydration creates a mechanically solid building material.
  • no portlandite Ca (OH) 2 is formed , it can not be detected by X-ray at any time.
  • the setting reaction proceeds with less heat release than with the hydration of Portland cement.
  • the setting speed can, as already known for Portland cement, by the substitution of various elements, the variation of the processing (eg grinding) and by surface-active additives, such as organic additives, set in a wide range.
  • the maximum of heat of hydration then decreases a period of a few minutes or only after several days.
  • the inventive hydraulic binder reacts to form a calcium silicate hydrate CSH phase.
  • the cross-linking of the silicate building units changes; at the macroscopic level, solidification takes place.
  • the hydration product optionally also contains further alkalis, alkaline earths or other elements, such that a calcium silicate hydrate having a molar Ca: Si ratio or a modified molar ratio [CaO + (x / 2) * ( M [6] x + O x / 2 )]: [SiO 2 + M [4] y + O y / 2 ] is smaller than 1.5.
  • Abboner Portland cement however, consists of a CSH gel (Ze mentgel) with a molar Ca: Si ratio of 1.7 to 1.8 and additionally contains Portlandit Ca (OH) 2 .
  • the building material resulting from the setting reaction according to the invention is more chemically resistant than Portland cement stone due to the lower molar Ca: Si ratio compared to cement stone from Portland cement and the higher linkage of the silicate building units.
  • the measured compressive strength after 28 days exceeds 20 N / mm 2 . This value is in the order of the European standard EN 197 for cements, which specifies 3 different classes for the strength of 32.5, 42.5 and 52.5 N / mm 2 .
  • the binder according to the invention contains less than 1% Na 2 O, it can be converted into a building material according to the invention together with alkali-sensitive additives, for example inorganic or organic fibers with low alkali resistance.
  • the production of the single-phase hydraulic binder according to the invention or of a mixture containing the single-phase hydraulic binder according to the invention is carried out by co-grinding (reaction milling) of an intermediate product, calcium, silicon and oxygen containing monomeric or dimeric silicate building units (ie, a calcium silicate), with a solid silicate raw material having a high degree of crosslinking, such as quartz or quartz sand.
  • the first starting material is characterized by the chemical elements calcium, silicon and oxygen, which are present in the form of monomeric or dimeric silicate units.
  • the second starting material is a silicate solid which is characterized by a high degree of crosslinking of the silicate tetrahedra of Q 3 to Q 4 .
  • small amounts of water can be added.
  • the single-phase hydraulic binder according to the invention results from milling the starting materials in a mill, preferably under increased shear and pressure, e.g. in a disc vibration mill, a ball mill or a roller mill.
  • the two reactants form a new substance with a medium degree of crosslinking.
  • the second starting material is depolymerized during co-grinding.
  • the single-phase binder thus formed contains silicate building units which, on the one hand, are kept in a storable state and, on the other hand, react hydraulically when the binder is mixed with water and lead to setting, to solidification.
  • the second starting material is quartz, quartz sand or another raw material, secondary raw material or a synthetic product.
  • Examples include silicate glasses, feldspars or slags.
  • Hydration products formed from a hydraulic binder according to the invention contain calcium silicate hydrates with a low molar Ca: Si ratio and are thus more chemically stable than CSH gels in Portland cement stone, since no Portlandite is formed and the silicate building units have a higher degree of crosslinking compared to Portland cement stone. Also, there is no weathering-sensitive portlandite at the contact points of the binder for aggregate in mortars or concretes, so that no predetermined breaking points in the composite of mortars and concretes form.
  • the binder according to the invention contains less than 1% Na 2 O, the binder framework formed therefrom is less susceptible to secondary alkali-silica reactions, so that alkali-sensitive additives can be used.
  • the starting materials were Belit ⁇ -Ca 2 SiO 4 and quartz, fine-grained, washed and calcined.
  • Belit was used according to the DE 10 2005 037 771 A1 from a mixture of CaCO 3 and SiO 2 in the ratio 2: 1 by multiple sintering at 1250 ° C and intermediate homogenization or by dehydration of hydrothermally produced ⁇ -Ca 2 SiO 4 ⁇ H 2 O prepared at 800 ° C.
  • Belit was then milled together with the quartz in a mass ratio of 1: 1 (1.1 g each) in a disk vibratory mill for 180 sec.
  • the grinding process primarily caused a reaction between the starting materials, which resulted in the formation of a hydraulic binder.
  • the BET surface area of the starting materials averaged 0.5 m 2 / g for belite and 2 m 2 / g for quartz, while the milled product had a value of 1.7 m 2 / g. If the starting materials were ground separately with the same weight and grinding time, the mean specific surface area was 5.2 m 2 / g. The common grinding thus led in reaction to form the binder of the invention, wherein the specific surface area has been reduced by about a factor of 3.
  • the hydration of the hydraulic binder was monitored by means of a thermal conductivity calorimeter. In this case, a maximum of the heat release due to the wetting heat a few seconds after dosing of the mixing water on. Thereafter, the heat release almost completely decayed, eventually rising to a minimum at about 25 minutes to a second maximum after about 10 hours. Over the next 100 hours, heat release slowly fades away. Although the reaction is associated with a lower heat release than the reaction of Portland cements, considerable strength is achieved within a few hours. With a ratio of water to binder of 0.3 and addition of three parts of sand to one part of binder, a compressive strength of 20 N / mm 2 was exceeded after 28 days.
  • the Q 2 -NMR signal which proves the appearance of the CSH phase, dominated the spectrum of the set building material. It was a clear one Intensity of the reflections in the powder diffractogram at 0.305 nm and 0.28 nm as well as the emergence of a broad reflection between 1.7 nm and 1.15 nm. This proves that the calcium-silicate hydrate is formed in the hardened building material. The location of the reflections indicates that the calcium silicate hydrate has a lower molar Ca: Si ratio than Portland Cement CSH gel.
  • the (Si-O) stretching vibration of the CSH phase was found to be 970 cm -1 , ie shifted to higher wavenumbers, which corresponds to a higher degree of crosslinking.
  • a new band was visible at 668 cm -1 . This corresponds to a Si-O-Si bending vibration, which is further evidence of the occurrence of a high polymer CSH phase.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Curing Cements, Concrete, And Artificial Stone (AREA)
  • Silicates, Zeolites, And Molecular Sieves (AREA)
EP08784792.7A 2007-07-27 2008-07-16 Einphasiges hydraulisches bindemittel, herstellungsverfahren und damit hergestellter baustoff Active EP2183193B1 (de)

Priority Applications (1)

Application Number Priority Date Filing Date Title
PL08784792T PL2183193T3 (pl) 2007-07-27 2008-07-16 Jednofazowe spoiwo hydrauliczne, sposób jego wytwarzania i wytworzony tym sposobem materiał budowlany

Applications Claiming Priority (2)

Application Number Priority Date Filing Date Title
DE102007035257A DE102007035257B3 (de) 2007-07-27 2007-07-27 Einphasiges hydraulisches Bindemittel, Verfahren zu seiner Herstellung und mit diesem Bindemittel hergestellter Baustoff
PCT/EP2008/005784 WO2009015769A1 (de) 2007-07-27 2008-07-16 Einphasiges hydraulisches bindemittel, herstellungsverfahren und damit hergestellter baustoff

Publications (2)

Publication Number Publication Date
EP2183193A1 EP2183193A1 (de) 2010-05-12
EP2183193B1 true EP2183193B1 (de) 2016-12-07

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US (1) US8382892B2 (pl)
EP (1) EP2183193B1 (pl)
JP (1) JP5496886B2 (pl)
KR (2) KR101621029B1 (pl)
CN (1) CN101835723B (pl)
AU (1) AU2008281031B2 (pl)
BR (1) BRPI0814133A2 (pl)
CA (1) CA2693512C (pl)
DE (1) DE102007035257B3 (pl)
EA (1) EA023687B1 (pl)
ES (1) ES2615162T3 (pl)
HU (1) HUE032561T2 (pl)
PL (1) PL2183193T3 (pl)
SG (1) SG183664A1 (pl)
TW (1) TWI496743B (pl)
WO (1) WO2009015769A1 (pl)
ZA (1) ZA200908734B (pl)

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DE102007035258B3 (de) * 2007-07-27 2008-11-20 Forschungszentrum Karlsruhe Gmbh Einphasiges hydraulisches Bindemittel, Verfahren zu seiner Herstellung und mit diesem Bindemittel hergestellter Baustoff
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CN101835723A (zh) 2010-09-15
HUE032561T2 (en) 2017-09-28
EP2183193A1 (de) 2010-05-12
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CA2693512A1 (en) 2009-02-05
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US20110041737A1 (en) 2011-02-24
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US8382892B2 (en) 2013-02-26
JP5496886B2 (ja) 2014-05-21
BRPI0814133A2 (pt) 2015-02-03
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KR20100040705A (ko) 2010-04-20
CA2693512C (en) 2015-07-14

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